气相色谱法分离测定丙烯酸-2-全氟烷基乙基酯  

Separation and determination of 2-perfluoroalkylethyl acrylates by Gas Chromatography

作　　者：施介华[1] 严巍[1] 王桂林[1] 王纪康[1] 

机构地区：[1]康浙江工业大学绿色化学合成技术国家重点实验室培育基地,浙江杭州310032

出　　处：《浙江工业大学学报》2009年第2期134-138,143,共6页Journal of Zhejiang University of Technology

基　　金：浙江省科技厅基金资助项目(2005C21121)

摘　　要：采用气相色谱在DB-5（30m×0．45mm×0．42μm）毛细柱上分离和测定丙烯酸-2-全氟烷基乙基酯．在所选定的色谱条件下，丙烯酸-2-全氟烷基乙基酯与内标物邻苯二甲酸二乙酯及杂质之间具有较好的分离效果．以邻苯二甲酸二乙酯为内标物时，CH2=CHCOOCH2CH2C6F13,CH2=CHCOOCH2CH2C8F17，CH2-CHCOOCH2CH2C10F21的校正因子（fω，A）分别为2．53，2．66，2．84，标准偏差分别为0．03，0．04，0．04．该方法具有操作简便、准确可靠．对同一试样的5次平行独立测定CH2=CHCOOCH2CH2C6F13，CH2=CHCOOCH2CH2C8F17，CH2=CHCOOCH2CH2C10F21的标准偏差分别为0．07％，0．44％和0．40％；相对标准偏差分别为0．88％，0．89％和1．85％；加入回收率分别为98．65％～101．0％，99．89％～102．6％和98．94％～99．87％．2-Perfluoroalkylethyl acrylates was separated and determined by gas chromatography on the DB-5 （30 m × 0.45 mm× 0. 42μm） capillary column. Under the selected chromatographic conditions, the high separation efficiency between 2-perfluoroalkylethyl acrylates, internal standard diethyl phthalate and impurities was achieved. Using diethyl phthalate as an internal standard, the correction factors of CH2 = CHCOOCH2 CH2 C6 F13, CH2 = CHCOOCH2 CH2 C8 F17 , CH2 =CHCOOCH2CH2C10F21 were 2.53, 2.66 and 2.84, and the standard deviations were 0.03, 0.04 and 0. 04, respectively. This is a simple, fast and accurate method for the determination of 2- perfluoroalkylethyl acrylates. Five-time tests of the same sample gave the mean value of 7.99%, 50.07% and 21. 32% with the standard deviation 0. 07%, 0. 44% and 0. 40%, the eoefficients of variation of 0. 88%, 0. 89 % and 1.85 %, and the recovery ratios of 98. 65 % （101.0%, 99.89% （102. 6%, 98. 94 % （99.87 % for the determination of CH2 = CHCOOCH2 CH2 C6 F13, CH2 = CHCOOCH2 CH2 C8 F17, CH2 = CHCOOCH2 CH2 C10 F21, respectively.

关 键 词：丙烯酸-2-全氟烷基乙基酯 中间体 气相色谱 

分 类 号：O657.7[理学—分析化学]